CN1966440B - Method for producing optical fiber probe - Google Patents
Method for producing optical fiber probe Download PDFInfo
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- CN1966440B CN1966440B CN200610144103A CN200610144103A CN1966440B CN 1966440 B CN1966440 B CN 1966440B CN 200610144103 A CN200610144103 A CN 200610144103A CN 200610144103 A CN200610144103 A CN 200610144103A CN 1966440 B CN1966440 B CN 1966440B
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Abstract
The invention disclosed a way to make optical fiber transducer which includes the following steps: 1) treating the quartz glass optical fiber which contains fiber core, wrapper and covering layer to make the wrapper of one end outerop; 2) dipping the outeropped end and its connected section which contains covering layer into the 10-30wt% fluohydric acid and let them react with each other. After the reaction, the rested covering layer of the quartz glass optical fiber outerops to get the cone fiber transducer. The invention has many advantages: easy to operate, low cost, easy to produce in quantity; the transducer has very good repeatability.
Description
Technical field
The present invention relates to a kind of method of making fibre-optical probe.
Background technology
Optical fiber is fibre-optic abbreviation.It is the soft filament that pulls into silica glass or tailormadepiston.Its typical structure is fibre core, covering and coat from inside to outside.The specific refractory power of covering is slightly less than the specific refractory power of fibre core, and by the total reflection principle of geometrical optics, light is restrainted to apply in fibre core to be transmitted.In the outside of covering is the coat of 5～40 μ m, and its effect is the physical strength that strengthens optical fiber, increases snappiness simultaneously.Outermost often has 100 μ m thick buffer layer or cover to mould layer.
Fibre-optical probe is the core component of optical fiber biosensor.Optical fiber biosensor since its have highly sensitive, biologic specificity is strong; Simple to operate, measuring speed is fast; Can monitor the dynamic process of biological respinse; Complete machine can miniaturization etc. characteristics, obtained using widely in biomedical research, food inspection, environmental monitoring, biological warfare agent field of detecting.The making of optical fiber biosensor fibre-optical probe at present is different and different according to material, if utilize plastic optical fiber to make probe, then normally adopts die methods; If utilize silica fibre, then normal employing is founded and is drawn the awl method and utilize stepper-motor in conjunction with chemical corrosion method.These methods need specific equipments such as expensive mould machine, pulling device and stepper-motor respectively, and the consistence of fibre-optical probe and repeatability are difficult to be guaranteed.On the other hand, how micromolecular compound is fixed to detecting head surface also is a difficult problem in the finishing field always.
Summary of the invention
The purpose of this invention is to provide a kind of method of making fibre-optical probe.
The method of making fibre-optical probe provided by the present invention may further comprise the steps:
1) handles quartz glass optical fibre (being designated hereinafter simply as silica fibre), the covering of one end is exposed with fibre core, covering and coat;
2) to place mass percent concentration be that 10～30% hydrofluoric acid solution reacts together with a section of coat of having that links to each other with described covering bared end with the covering bared end of described silica fibre, residue clad section with described silica fibre after reaction finishes exposes, and obtains tapered fibre-optical probe.
In order to make hydrofluoric acid and SiO
2Speed of reaction moderate, the mass percent concentration of described hydrofluoric acid solution is preferably 30%.
When the structure of described silica fibre is fibre core, covering and coat from inside to outside; By the coat of removing described silica fibre one end the covering of described silica fibre one end is exposed in the described step 1), described step 2) after reaction finished in, the coat by removing the described silica fibre the other end exposed the residue clad section of described silica fibre.
When the structure of described silica fibre is moulded layer for fibre core, covering, coat and cover from inside to outside; Moulding layer by the coat of removing described silica fibre one end with cover in the described step 1) exposes the covering of described silica fibre one end, described step 2) after reaction finished in, coat by removing the described silica fibre the other end and cover were moulded layer the residue clad section of described silica fibre are exposed.
When the structure of described silica fibre is fibre core, covering, coat and buffer layer from inside to outside; By coat and the buffer layer of removing described silica fibre one end the covering of described silica fibre one end is exposed in the described step 1), described step 2) after reaction finished in, coat by removing the described silica fibre the other end and buffer layer exposed the residue clad section of described silica fibre.
The temperature of reaction of described reaction can be 20～35 ℃.
In the aforesaid method, the surface of described fibre-optical probe is fixed with organic micromolecule compound; Described organic micromolecule compound can be fixed to described fibre-optical probe surface according to the method that comprises the steps: the conjugate that 1) organic micromolecule compound and the coupling of inert protein molecule is obtained organic micromolecule compound and inert protein molecule; With described fibre-optical probe silanization; 2) conjugate of described organic micromolecule compound and inert protein molecule is connected to the surface of described silanization fibre-optical probe by bifunctional reagent.
Described inert protein molecule can be bovine serum albumin, ovalbumin, human serum albumin or hemocyanin.
Because organic micromolecule compound is diversified, so it and inert protein molecule link coupled method also are different, existing coupling method all can adopt, as: EDC (carbodiimide) method: EDC at first and hapten molecule (as: 2, carboxyl reaction 4-D) generates an addition intermediate product, again with the inert protein molecule on amino-acid residue reaction form amido linkage, realize the covalent attachment of haptens and carrier proteins; Glutaraldehyde method: (albumen: glutaraldehyde is 1: 500-1000) at first to use excessive glutaraldehyde and albumen test, remove unnecessary glutaraldehyde with Sephadex G-25 chromatography column then, make activated protein (albumen-glutaraldehyde mixture), add a certain amount of small molecules again, remaining aldehyde radical on the activated protein is combined with amino on the small molecules, make coupled product.
Described organic micromolecule compound can be existing micromolecular compound, as 2,4 dichlorophenoxyacetic acid, G-30027 or algae toxin etc.
Described bifunctional reagent is γ-dimaleoyl imino butyric acid-N-hydroxy-succinamide acid (GMBS).
The present invention is corroded silica fibre with hydrofluoric acid, utilize capillary action, make in the tube chamber of hydrofluoric acid solution between coat and covering and form microconvection, corrosion process is upwards reaction step by step in this columniform pipe, forms the fibre-optical probe with certain coning angle after after a while.
The present invention utilizes capillary action, successfully produces the tapered fibre-optical probe of high-quality combination, and this making method is easy to operate, and is with low cost, is easy to produce in batches, and the fibre-optical probe of making has good repetition rate.Simultaneously, the present invention combines micromolecular compound earlier with the inert protein molecule, then this mixture successfully is connected on the fibre-optical probe surface behind the silanization by bifunctional reagent, the density of fibre-optical probe surface micromolecular compound has reached the requirement of subsequent detection.
Further set forth the present invention below in conjunction with the drawings and specific embodiments.
Description of drawings
Fig. 1 is the making processes synoptic diagram of the tapered fibre-optical probe of combination
Fig. 2 is the tapered fibre-optical probe synoptic diagram of combination
Fig. 3 is a fibre-optical probe finishing process synoptic diagram
Embodiment
1, the making of fibre-optical probe
Can make fibre-optical probe according to following method:
As shown in Figure 1, cut the fiber segment that optical fiber is cut into desired length with the optical fiber special use earlier, polish and polish with the end of optic fiber polishing machine then optical fiber.From the other end of fiber segment the plastics jacket layer 1 usefulness special vice of optical fiber surface is removed approximately 1/2 again, and the coat 3 of this part rejected with blade carefully, the covering of fibre core and covering 2 is exposed.
The a certain amount of mass concentration of packing in plastic containers earlier is 10～30% hydrofluoric acid, covers the plastic bottle closure of have openning hole (being generally 6～10).Insert in these plastic containers the part of the removal plastics jacket layer 1 of the above-mentioned fiber segment of handling well and coat 3 is vertical down then, the fiber segment that is not removed plastics jacket layer 1 and coat 3 until part is submerged in the hydrofluoric acid, wherein is not removed the degree of depth that the fiber segment of plastics jacket layer 1 and coat 3 partly immerses in the hydrofluoric acid and decides according to the length of the tapered part 22 of the tapered fibre-optical probe of required combination.At this moment, the fiber segment part exposed of coat covering that acid solution has begun erosion removal, but can not react with coat, this overcoat has played the effect of similar protective wall, protects other not have the part of crevice corrosion liquid.Under the protection of this coat; because capillary action; form microconvection in the tube chamber of hydrofluoric acid solution between coat and covering; corrosion process is upwards reaction step by step in this columniform pipe; formation is had after after a while the fibre-optical probe of certain coning angle, at last plastics jacket layer 1 and coat 3 are removed the tapered fibre-optical probe of the combination that can obtain as shown in Figure 2.This makes up tapered fibre-optical probe and is made up of be not corroded part 21, probe tapered part 22 and the responsive part 23 of popping one's head in of probe.
Under certain envrionment temperature, can decide required etching time according to the size of required corrosion back optical fiber core diameter 23.
2, micromolecular compound is fixing
Normally micromolecular compound is fixed on responsive part 23 surfaces of fibre-optical probe,, should cleans the surface of fibre-optical probe earlier for reaching this purpose.Preparation Piranha solution [dense H
2SO
4: H
2O
2=7: 3 (volume ratios)], above-mentioned fibre-optical probe is immersed wherein 30min; Putting into ultrasonic washing instrument then and wash, and fully clean with ultrapure water, is neutral up to the pH of scavenging solution value, at room temperature dries up with nitrogen at last, is stored in the vacuum drying oven standby.
With haptens small molecules derivative (as 2, carboxyl 4-D) and carbodiimide (EDC) reaction generates an addition intermediate product, again with inert support protein molecular (as BSA, OVA etc.) on amino-acid residue reaction form amido linkage, realize the covalent attachment of haptens and carrier proteins, synthetic bag is by the mixture of micromolecular compound.
For micromolecular compound is connected on the probe, see also Fig. 3, earlier with the fibre-optical probe silanization, the fibre-optical probe of cleaning put into to contain the quality percentage composition be that the toluene solution of 2%3-sulfydryl propyl trimethoxy silicane (MTS) reacts 2h.Clean three times with toluene solution, putting into concentration then is 0.02M bifunctional reagent γ-dimaleoyl imino butyric acid-N-hydroxy-succinamide acid, be in the ethanolic soln of N-(4-Maleimidobutyryloxy) succinimide (GMBS), use alcohol flushing three times behind the reaction 1h, rinse well with PBS again, at last that silanization is good fibre-optical probe puts into the 0.05mg/ml small molecules and the inert protein mixture reacts 2h, after the PBS flushing, preserves standby at 4 ℃ of refrigerators.
The making of embodiment 1, the tapered fibre-optical probe of combination
As Fig. 1, earlier with the optical fiber special use cut with core diameter be 600 μ m, covering thick be the fiber segment that the optical fiber (Nanjing light of spring Scientific and Technical Industry Co., Ltd) of 10 μ m is cut into 11cm length, polish with the end of optical fiber grinding equipment then, and polish with polishing machine with optical fiber.From the end that do not polish of fiber segment the plastics jacket layer 1 usefulness special vice of optical fiber surface is removed 6.3cm again, at last the coat 3 of this part is rejected with blade carefully, the covering of fibre core and covering 2 is exposed.
The part of the removal plastics jacket layer 1 of the above-mentioned fiber segment of handling well and coat 3 inserted down be equipped with in hydrofluoric acid (mass percentage concentration of HF the is 30%) solution, immersion depth is 7.3cm, and etching time is 180min.Obtain tapered fibre-optical probe as shown in Figure 2, it is 220 μ m that the diameter of the responsive part 23 of promptly popping one's head in is held in corrosion, and the length of tapered part 22 is 0.5cm.The coning angle of this tapered fibre-optical probe is 0.37.
Mass percentage concentration is that 30% hydrofluoric acid solution is (600+10-220) μ m/180min=2.17 μ m/min to fibre core and covering 2 at the radial average corrosion rate.
The making of embodiment 2, the tapered fibre-optical probe of combination
As Fig. 1, earlier with the optical fiber special use cut with core diameter be 600 μ m, covering thick be the fiber segment that the optical fiber (Nanjing light of spring Scientific and Technical Industry Co., Ltd) of 10 μ m is cut into 11cm length, polish with the end of optical fiber grinding equipment then, and polish with polishing machine with optical fiber.From the end that do not polish of fiber segment the plastics jacket layer 1 usefulness special vice of optical fiber surface is removed 6.3cm again, at last the coat 3 of this part is rejected with blade carefully, the covering of fibre core and covering 2 is exposed.
The part of the removal plastics jacket layer 1 of the above-mentioned fiber segment of handling well and coat 3 inserted down be equipped with in hydrofluoric acid (mass percentage concentration of HF the is 20%) solution, immersion depth is 7.3cm, and etching time is 240min.Obtain tapered fibre-optical probe as shown in Figure 2, it is 230 μ m that the diameter of the responsive part 23 of promptly popping one's head in is held in corrosion, and the length of tapered part 22 is 0.5cm.The coning angle of this tapered fibre-optical probe is 0.38.
Mass percentage concentration is that 20% hydrofluoric acid solution is (600+10-230) μ m/240min=1.58 μ m/min to fibre core and covering 2 at the radial average corrosion rate.
The making of embodiment 3, the tapered fibre-optical probe of combination
As Fig. 1, earlier with the optical fiber special use cut with core diameter be 600 μ m, covering thick be the fiber segment that the optical fiber (Nanjing light of spring Scientific and Technical Industry Co., Ltd) of 10 μ m is cut into 11cm length, polish with the end of optical fiber grinding equipment then, and polish with polishing machine with optical fiber.From the end that do not polish of fiber segment the plastics jacket layer 1 usefulness special vice of optical fiber surface is removed 6.3cm again, at last the coat 3 of this part is rejected with blade carefully, the covering of fibre core and covering 2 is exposed.
The part of the removal plastics jacket layer 1 of the above-mentioned fiber segment of handling well and coat 3 inserted down be equipped with in hydrofluoric acid (mass percentage concentration of HF the is 10%) solution, immersion depth is 7.3cm, and etching time is 360min.Obtain tapered fibre-optical probe as shown in Figure 2, it is 230 μ m that the diameter of the responsive part 23 of promptly popping one's head in is held in corrosion, and the length of tapered part 22 is 0.5cm.The coning angle of this tapered fibre-optical probe is 0.38.
Mass percentage concentration is that 20% hydrofluoric acid solution is (600+10-230) μ m/360min=1.05 μ m/min to fibre core and covering 2 at the radial average corrosion rate.
The consistence of embodiment 4, fibre-optical probe
For investigating the difference between the different fiber probe, picked at random be 0.37 fibre-optical probe according to 5 root angle degree of the method for embodiment 1 preparation, non-corrosion part 21 with fibre-optical probe is connected with biologic sensor for fast travelling waves of optical fibre respectively, and it is 4 * 10 that the responsive part 23 of fibre-optical probe is put into concentration respectively
-8, 1 * 10
-8, 2 * 10
-9In mol/1 fluorescence dye (Cy5.5) solution, the fluorescence intensity of detection fiber probe, each concentration duplicate detection 3 times is got its mean value, and the result who obtains is as shown in table 1.
The consistence of table 1 fibre-optical probe
Table 1 shows to have good consistence between the fibre-optical probe, and relative standard deviation is no more than 2%, and this haves laid a good foundation for later experiment.
1, preparation 2,4-D-BSA
(2, carboxyl 4-D) and carbodiimide (EDC) reaction generates an addition intermediate product with 2,4 dichlorphenoxyacetic acids, again with carrier proteins molecule BSA on amino-acid residue reaction form amido linkage, realize the covalent attachment of haptens and carrier proteins, synthetic envelope antigen 2,4-D-BSA.Concrete preparation method is as follows: compound concentration is the phosphate buffer soln of 0.05mol/L, is 11 with the salt acid for adjusting pH value.With this phosphate buffered saline buffer compound concentration is 12mg/mL 2, and the solution of 4-D is 5.4 with the pH of hydrochloric acid conditioning solution.Above-mentioned 2 at 2.5mL, adding 100 μ L concentration in the 4-D damping fluid respectively is the BSA solution of 50mg/mL, adds 15mg EDC again and stirs gently simultaneously.4 ℃ left standstill 18 hours.With 0.1mol/L NaHCO
3The solution dialysis gets final product.
2, the silanization of fibre-optical probe
For with small molecules 2,4-D is connected on the fibre-optical probe, and as Fig. 3, earlier with the fibre-optical probe silanization, concrete grammar is as follows: the fibre-optical probe according to the preparation of embodiment 2 methods of cleaning is put into to contain the quality percentage composition be that the toluene solution of 2% MTS reacts 2h.Clean three times with toluene solution, obtain the fibre-optical probe of silanization.
3,2,4 dichlorophenoxyacetic acid is fixed on the surface of fibre-optical probe
The fibre-optical probe of silanization is put into 0.02M GMBS ethanolic soln, use alcohol flushing three times behind the reaction 1h, put into 0.05mg/ml 2 after rinsing well with PBS again, react 2h in the 4-D-BSA aqueous solution, with the PBS flushing, obtain the surface and be fixed with 2,4 dichlorophenoxyacetic acid fixed fibre-optical probe.After testing, 2 of this fibre-optical probe surface, the concentration of 4-D is 3nmol/cm
2, reached the requirement of subsequent detection.
Claims (9)
1. ten thousand methods of making fibre-optical probe may further comprise the steps:
1) handles quartz glass optical fibre, the covering of one end is exposed with fibre core, covering and coat;
2) to place mass percent concentration be that 10～30% hydrofluoric acid solution reacts together with a section of coat of having that links to each other with described covering bared end with the covering bared end of described quartz glass optical fibre, residue clad section with described quartz glass optical fibre after reaction finishes exposes, and obtains tapered fibre-optical probe.
2. method according to claim 1 is characterized in that: the mass percent concentration of described hydrofluoric acid solution is 30%.
3. method according to claim 1 is characterized in that: the structure of described quartz glass optical fibre is fibre core, covering and coat from inside to outside;
By the coat of removing described quartz glass optical fibre one end the covering of described quartz glass optical fibre one end is exposed in the described step 1); Described step 2) after reaction finished in, the coat by removing the described quartz glass optical fibre the other end exposed the residue clad section of described quartz glass optical fibre.
4. method according to claim 1 is characterized in that: the structure of described quartz glass optical fibre is moulded layer for fibre core, covering, coat and cover from inside to outside;
Moulding layer by the coat of removing described quartz glass optical fibre one end with cover in the described step 1) exposes the covering of described quartz glass optical fibre one end; Described step 2) after reaction finished in, coat by removing the described quartz glass optical fibre the other end and cover were moulded layer the residue clad section of described quartz glass optical fibre are exposed.
5. method according to claim 1 is characterized in that: the structure of described quartz glass optical fibre is fibre core, covering, coat and buffer layer from inside to outside;
By coat and the buffer layer of removing described quartz glass optical fibre one end the covering of described quartz glass optical fibre one end is exposed in the described step 1); Described step 2) after reaction finished in, coat by removing the described quartz glass optical fibre the other end and buffer layer exposed the residue clad section of described quartz glass optical fibre.
6. according to arbitrary described method in the claim 1 to 5, it is characterized in that: the temperature of reaction of described reaction is 20-35 ℃.
7. according to arbitrary described method in the claim 1 to 5, it is characterized in that: the surface of described fibre-optical probe is fixed with organic micromolecule compound; Described organic micromolecule compound is fixed to described fibre-optical probe surface according to the method that comprises the steps: the conjugate that 1) organic micromolecule compound and the coupling of inert protein molecule is obtained organic micromolecule compound and inert protein molecule; With described fibre-optical probe silanization; 2) conjugate of described organic micromolecule compound and inert protein molecule is connected to the surface of described silanization fibre-optical probe by bifunctional reagent; Described bifunctional reagent is γ-dimaleoyl imino butyric acid-N-hydroxy-succinamide acid.
8. method according to claim 7 is characterized in that: described inert protein molecule is bovine serum albumin, ovalbumin, human serum albumin or hemocyanin.
9. method according to claim 7 is characterized in that: described organic micromolecule compound is 2,4 dichlorophenoxyacetic acid, G-30027 or algae toxin.
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|---|---|---|---|
| CN200610144103A CN1966440B (en) | 2006-11-27 | 2006-11-27 | Method for producing optical fiber probe |
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|---|---|---|---|
| CN200610144103A CN1966440B (en) | 2006-11-27 | 2006-11-27 | Method for producing optical fiber probe |
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| CN1966440B true CN1966440B (en) | 2010-05-12 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP4166060A3 (en) * | 2016-12-22 | 2023-07-26 | Magic Leap, Inc. | Methods and systems for fabrication of shaped fiber elements for scanning fiber displays |
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| CN103896484B (en) * | 2012-12-28 | 2016-08-03 | 清华大学 | Optical taper district manufacture method and device |
| CN103197380B (en) * | 2013-03-27 | 2015-03-25 | 合肥工业大学 | Preparation method of contact-type optical fiber micro probe based on optical fiber tapering technology |
| CN105424663A (en) * | 2015-11-24 | 2016-03-23 | 西南大学 | Method for detecting phthalic acid ester compound concentration based on optical fiber immunosense |
| CN105738007A (en) * | 2016-02-03 | 2016-07-06 | 西安交通大学 | Biconical polymer optical fiber probe and preparation method thereof and temperature sensor |
| CN106596480B (en) * | 2016-12-01 | 2020-03-10 | 中国人民大学 | Mercury ion nano sensor and preparation method and application thereof |
| CN107056092A (en) * | 2017-05-25 | 2017-08-18 | 清华大学 | A kind of etching solution for preparing microscratch conical fiber sensing probe |
| CN108732388A (en) * | 2018-03-30 | 2018-11-02 | 姜全博 | A kind of production method of single-photon source active probe |
| CN109455955A (en) * | 2018-10-23 | 2019-03-12 | 华侨大学 | A kind of U-shaped fibre-optical probe preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1146811A (en) * | 1994-04-22 | 1997-04-02 | 艾利森电话股份有限公司 | Fibre reflector |
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2006
- 2006-11-27 CN CN200610144103A patent/CN1966440B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1146811A (en) * | 1994-04-22 | 1997-04-02 | 艾利森电话股份有限公司 | Fibre reflector |
Non-Patent Citations (2)
| Title |
|---|
| 杨修文等.STM光纤探针的研制.光电子技术22 9.2002,22(9),153-155. |
| 杨修文等.STM光纤探针的研制.光电子技术22 9.2002,22(9),153-155. * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP4166060A3 (en) * | 2016-12-22 | 2023-07-26 | Magic Leap, Inc. | Methods and systems for fabrication of shaped fiber elements for scanning fiber displays |
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